CN114685881B - Flame-retardant LLDPE/EVA composite material and preparation method and application thereof - Google Patents
Flame-retardant LLDPE/EVA composite material and preparation method and application thereof Download PDFInfo
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- CN114685881B CN114685881B CN202210318008.7A CN202210318008A CN114685881B CN 114685881 B CN114685881 B CN 114685881B CN 202210318008 A CN202210318008 A CN 202210318008A CN 114685881 B CN114685881 B CN 114685881B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a flame-retardant LLDPE/EVA composite material, and a preparation method and application thereof. The flame-retardant LLDPE/EVA composite material comprises the following components in parts by weight: 30-50 parts of linear low-density polyethylene, 20-45 parts of metallocene polyethylene, 15-30 parts of ethylene-vinyl acetate copolymer, 5-10 parts of phosphate halogen-free flame retardant and 2-10 parts of synergistic auxiliary agent; the phosphate halogen-free flame retardant is one or more of hypophosphite, pyrophosphate or polyphosphate, and the synergistic auxiliary agent is one or more of nylon resin, epoxy resin or phenolic resin. The phosphate halogen-free flame retardant and a specific synergistic auxiliary agent cooperate, and meanwhile, the synergistic auxiliary agent also plays a role in improving the tearing strength of the material, the flame retardant grade of the flame retardant LLDPE/EVA composite material reaches V0 grade, the oxygen index is more than or equal to 30, and the tearing strength is more than or equal to 100KN/m.
Description
Technical Field
The invention relates to the technical field of waterproof materials, in particular to a flame-retardant LLDPE/EVA composite material, and a preparation method and application thereof.
Background
Polyolefin materials such as Linear Low Density Polyethylene (LLDPE) and ethylene-vinyl acetate copolymer (EVA) have excellent low water permeability, low-temperature flexibility, ductility and processability, and the extruded sheet is very suitable for building inner and outer waterproofing. However, because polyethylene and EVA materials are all inflammable materials, the polyethylene and EVA materials are easy to be ignited at high temperature caused by welding slag or short circuit of electric lines and the like in the construction and use processes of roof photovoltaic power stations, tunnels or underground buildings, and have great potential safety hazards in closed or semi-closed spaces, the requirement on fireproof safety is high, and flame retardant modification is needed for waterproof materials.
The prior art reports a flame-retardant waterproof sheet with high puncture resistance and high polarity and a preparation method thereof, wherein the adopted flame retardant is a bromine-antimony flame retardant, and has certain flame retardant property, but the flame retardant contains bromine, so that a large amount of smoke and toxic hydrogen bromide gas can be generated when the material is combusted, and the safety performance of the flame-retardant waterproof sheet can not meet the smoke toxicity standard of building materials.
In order to solve the problem of the bromine-containing flame retardant, the prior art discloses a low-smoke halogen-free environment-friendly EVA/LLDPE flame-retardant composite material, which adopts metal hydroxide, such as aluminum hydroxide and magnesium hydroxide, as the halogen-free flame retardant to improve the flame retardance of the composite material. However, metal hydroxides have a relatively low flame retardant efficiency and generally require a relatively large amount of additions to achieve V0 flame retardant rating. And the excessive addition amount causes the problems that the mechanical property of the flame retardant material is poor, particularly the tearing strength is poor, the sharp hard objects are easy to puncture and tear in the construction process, and the waterproof and anti-permeability performance is greatly reduced.
Therefore, there is a need to develop a flame retardant LLDPE/EVA composite material that combines excellent flame retardancy and tear strength.
Disclosure of Invention
The invention provides a flame-retardant LLDPE/EVA composite material, which aims to overcome the defect of poor tear resistance in the prior art, and the flame-retardant property of the composite material is obviously improved through the synergistic effect of a phosphate halogen-free flame retardant and a specific synergistic auxiliary agent, so that the flame-retardant grade is V0 grade, and the oxygen index is more than or equal to 30; on one hand, the synergistic auxiliary agent is favorable for the char formation of the material and the stability of the char layer, plays a role in flame retardation and synergistic effect, and ensures that the adding proportion of the phosphate halogen-free flame retardant is smaller, so that the influence on the mechanical property of the material is smaller; on the other hand, the synergistic auxiliary agent can also form a net structure, so that the tearing performance of the material is improved, and the flame-retardant LLDPE/EVA composite material has higher tearing strength.
Another object of the present invention is to provide a method for preparing the above flame retardant LLDPE/EVA composite material.
It is another object of the present invention to provide the use of the flame retardant LLDPE/EVA composite material described above.
In order to solve the technical problems, the invention adopts the following technical scheme:
a flame-retardant LLDPE/EVA composite material comprises the following components in parts by weight:
30 to 50 parts of Linear Low Density Polyethylene (LLDPE),
20 to 45 parts of metallocene polyethylene (m-PE),
15-30 parts of ethylene-vinyl acetate copolymer (EVA),
5-10 parts of phosphate halogen-free flame retardant;
2-10 parts of synergistic auxiliary agent; the phosphate halogen-free flame retardant is one or more of hypophosphite, pyrophosphate or polyphosphate;
the synergistic auxiliary agent is one or more of nylon resin, epoxy resin or phenolic resin.
In the thermal degradation or combustion process of the material, the phosphate halogen-free flame retardant plays a role in flame retardance of gas phase and condensed phase in the combustion process. The phosphorus-containing organic free radicals neutralize free radicals generated by polypropylene decomposition, so that the flame retardant effect of a gas phase is achieved, the penetration of heat and combustible gas is effectively blocked by the vitreous fused phosphate, and the polyphosphoric acid generated by decomposition has the dehydration and char forming effects, so that the flame retardant effect of a condensed phase is achieved. And the water vapor produced by combustion absorbs a large amount of heat, thereby reducing the combustion temperature and the heat release rate.
The synergistic auxiliary agent is one or more of nylon resin, epoxy resin or phenolic resin, and is a polymer material containing a large amount of amide or ester functional groups. In the combustion process of the composite material, the synergistic auxiliary agent is favorable for the carbon formation and the carbon layer stabilization of the material, and plays a role in synergistic flame retardance with the phosphate halogen-free flame retardant, so that the addition amount of the phosphate halogen-free flame retardant can be greatly reduced, the addition proportion of the phosphate halogen-free flame retardant is smaller, and the influence on the mechanical property of the material is smaller. In addition, in the processing process of the composite material, the synergistic auxiliary agent forms a net structure in LLDPE/EVA matrix resin through the shearing action of a screw rod, and the tearing performance of the material is improved, so that the flame-retardant LLDPE/EVA composite material has higher tearing strength.
In addition, in the LLDPE/EVA system, the phosphate halogen-free flame retardant and the synergistic auxiliary agent have better compatibility with LLDPE and EVA. The flame retardant grade of the flame retardant LLDPE/EVA composite material reaches V0 grade and the oxygen index reaches more than 30 through the synergistic effect of the phosphate halogen-free flame retardant and the synergistic auxiliary agent; the synergistic auxiliary agent also plays a role in improving the tearing strength of the material, and the tearing strength of the flame-retardant LLDPE/EVA composite material is more than or equal to 100KN/m.
Preferably, the phosphate type halogen-free flame retardant is hypophosphite.
Compared with pyrophosphates or polyphosphates, the hypophosphite has better compatibility with organic resins in LLDPE/EVA systems, better reactivity and better flame retardant effect.
Optionally, the hypophosphite is one or more of aluminum hypophosphite, calcium hypophosphite, ammonium hypophosphite or hypophosphite.
Preferably, the metallocene polyethylene has a melt flow rate of 0.5 to 5g/10min at 190℃under 2.16 kg.
Preferably, the linear low density polyethylene has a melt flow rate of 2 to 30g/10min at 190℃under 2.16 kg.
Preferably, the synergistic auxiliary agent is nylon resin.
Optionally, the nylon resin is one or more of PA66, PA6T, PA10, PA11 or PA 12.
Optionally, the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, epoxidized olefin compound or heterocyclic epoxy resin.
Optionally, the phenolic resin is a thermoplastic phenolic resin and/or a thermosetting phenolic resin.
Preferably, the VA content in the EVA is 8 to 40wt.%.
Preferably, the flame retardant LLDPE/EVA composite material can further comprise 0.1-2 parts by weight of compatilizer and 0.1-2 parts by weight of lubricant.
The invention also provides a preparation method of the flame-retardant LLDPE/EVA composite material, which comprises the following steps:
mixing linear low density polyethylene, ethylene-vinyl acetate copolymer, metallocene polyethylene, phosphate halogen-free flame retardant, synergistic auxiliary agent, compatilizer (if any) and lubricant (if any), adding into an extruder, melting, mixing, extruding and granulating to obtain the flame-retardant LLDPE/EVA composite material.
Preferably, the extruder is a twin screw extruder.
More preferably, the length-diameter ratio of the screws of the double screw extruder is 36-52:1, and the melting temperature is 150-200 ℃.
The invention also protects the application of the flame-retardant LLDPE/EVA composite material in roof photovoltaic power station waterproofing, tunnel waterproofing and underground building waterproofing.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops a flame-retardant LLDPE/EVA composite material. The phosphate halogen-free flame retardant and a specific synergistic auxiliary agent cooperate to enable the flame retardant grade of the flame retardant LLDPE/EVA composite material to reach V0 grade and the oxygen index to reach more than 30; the synergistic auxiliary agent also plays a role in improving the tearing strength of the material, and the tearing strength of the flame-retardant LLDPE/EVA composite material is more than or equal to 100KN/m.
Detailed Description
The invention is further described below in connection with the following detailed description.
The raw materials in examples and comparative examples are all commercially available, and are specifically as follows:
unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Examples 1 to 17
Examples 1-17 respectively provide a flame retardant LLDPE/EVA composite material, the component contents are shown in Table 1, and the preparation method is as follows:
adding the components into a double-screw extruder according to the table 1, and carrying out melt mixing at 150-200 ℃ and extrusion granulation to obtain a flame-retardant LLDPE/EVA composite material; wherein the screw length-diameter ratio of the twin-screw extruder is 48:1.
Table 1 the content of components (parts by weight) of flame retardant LLDPE/EVA composite materials of examples 1 to 17
Comparative examples 1 to 6
Comparative examples 1 to 6 respectively provide a flame retardant LLDPE/EVA composite material, the component contents are shown in Table 1, and the preparation method is as follows:
adding the components into a double-screw extruder according to the table 1, and carrying out melt mixing at 150-200 ℃ and extrusion granulation to obtain a flame-retardant LLDPE/EVA composite material; wherein the screw length-diameter ratio of the twin-screw extruder is 48:1.
Table 2 component content (parts by weight) of flame retardant LLDPE/EVA composite materials of comparative examples 1 to 6
Performance testing
The performance test is carried out on the flame retardant LLDPE/EVA composite materials prepared in the examples and the comparative examples, and the specific method is as follows:
tear strength: testing according to GB/T529-2008 standard method;
flame retardant rating: the sample strip is tested according to the UL94-1985 standard method and has the specification of 2.0 mm;
oxygen index: tested according to GBT2406.1-2008 standard.
The test results of the examples and comparative examples are shown in tables 3 and 4, respectively.
Table 3 test results of examples
According to the test results of Table 3, the flame retardant LLDPE/EVA composite material prepared by each embodiment of the invention has excellent flame retardant property, the flame retardant grade is V0, the oxygen index is more than or equal to 30, the tear resistance is good, and the tear strength is more than or equal to 100KN/m.
In examples 1-4, the oxygen index of the flame retardant LLDPE/EVA composites of examples 1, 2 was relatively higher, indicating that their flame retardant properties were relatively better. It can be seen that when the phosphate halogen-free flame retardant is hypophosphite, the material has better flame retardant property.
According to examples 1, 5-10, the melt flow rate of the metallocene polyethylene at 190℃under 2.16kg is preferably 0.5-3 g/10min, the melt flow rate of the linear low density polyethylene at 190℃under 2.16kg is preferably 2-30 g/10min, and the VA content in the EVA is preferably 8-40 wt.%.
According to examples 1, 11 and 12, nylon resin, epoxy resin or phenolic resin can be used as a synergistic auxiliary agent to achieve synergistic flame retardant effect with phosphate halogen-free flame retardant and improve the tearing strength of the material. Wherein the oxygen index and tear strength of the flame retardant LLDPE/EVA composite material of example 1 are higher, the synergistic auxiliary agent is preferably nylon resin.
Table 4 test results of comparative examples
The flame retardant used in comparative example 1 was magnesium hydroxide, and at an additive amount of 5 parts by weight, the flame retardant LLDPE/EVA composite material was poor in flame retardant effect, and the oxygen index was only 20. The addition amount of the flame retardant magnesium hydroxide in comparative example 2 was increased to 50 parts by weight, and the flame retardant property of the material was improved, the flame retardant rating reached V0, and the oxygen index reached 38, but the mechanical property of the material was severely deteriorated, and the tear strength was only 46KN/m.
In comparative examples 3 and 4, the flame retardant contained phosphorus, but was not the same as in the embodiment of the present invention. It can be seen that red phosphorus or ammonium phosphate flame retardants have poor flame retardant effect in LLDPE/EVA systems.
In the comparative example 5, no synergistic auxiliary agent is added, the flame retardant performance of the flame retardant LLDPE/EVA composite material is obviously reduced compared with that of the example 1, and it can be seen that under the condition of no synergistic auxiliary agent, the phosphate halogen-free flame retardant acts independently, so that a good flame retardant effect cannot be brought to the material; and the tear resistance of the flame retardant LLDPE/EVA composite material is also poor.
In comparative example 6, polytetrafluoroethylene is used for replacing the synergistic auxiliary agent of the invention in an equivalent manner, and the tear strength of the material can be better improved, but the synergistic flame retardant performance with the phosphate halogen-free flame retardant is poorer, and the flame retardant grade of the prepared flame retardant LLDPE/EVA composite material can only reach V2.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (10)
1. The flame-retardant LLDPE/EVA composite material is characterized by comprising the following components in parts by weight:
30 to 50 parts of linear low-density polyethylene,
20 to 45 parts of metallocene polyethylene,
15-30 parts of ethylene-vinyl acetate copolymer,
5-10 parts of phosphate halogen-free flame retardant;
2-10 parts of synergistic auxiliary agent;
the phosphate halogen-free flame retardant is one or more of hypophosphite, pyrophosphate or polyphosphate;
the synergistic auxiliary agent is one or more of nylon resin, epoxy resin or phenolic resin;
the nylon resin is one or more of PA66, PA6T, PA10, PA11 or PA 12; the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, epoxy olefin compound or heterocyclic epoxy resin; the phenolic resin is thermoplastic phenolic resin and/or thermosetting phenolic resin.
2. The flame retardant LLDPE/EVA composite of claim 1, wherein said phosphate-based halogen-free flame retardant is hypophosphite.
3. The flame retardant LLDPE/EVA composite of claim 1 or 2, wherein said hypophosphite is one or more of aluminum hypophosphite, calcium hypophosphite, ammonium hypophosphite or phosphinate.
4. The flame retardant LLDPE/EVA composite of claim 1, wherein said metallocene polyethylene has a melt flow rate of 0.5 to 5g/10min at 190 ℃ under 2.16kg conditions.
5. The flame retardant LLDPE/EVA composite of claim 1, wherein said linear low density polyethylene has a melt flow rate of 2 to 30g/10min at 190 ℃ under 2.16kg conditions.
6. Flame retardant LLDPE/EVA composite according to claim 1, wherein the VA content in the EVA is 8-40 wt.%.
7. The flame retardant LLDPE/EVA composite of claim 1, wherein said co-efficient auxiliary is a nylon resin.
8. The flame retardant LLDPE/EVA composite material according to claim 1, wherein the flame retardant LLDPE/EVA composite material further comprises 0.1-2 parts by weight of a compatilizer and 0.1-2 parts by weight of a lubricant.
9. The method for preparing a flame retardant LLDPE/EVA composite material as claimed in any one of claims 1 to 7, comprising the steps of:
mixing linear low-density polyethylene, ethylene-vinyl acetate copolymer, metallocene polyethylene, phosphate halogen-free flame retardant and synergistic auxiliary agent, adding the mixture into an extruder, and carrying out melt mixing, extrusion granulation to obtain the flame-retardant LLDPE/EVA composite material.
10. Use of the flame retardant LLDPE/EVA composite of any one of claims 1 to 8 in roofing photovoltaic power station waterproofing, tunnel waterproofing, and waterproofing of underground construction.
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